CN101235289A - Water-phase synthesis method for water-soluble CdZnTe ternary quantum dots - Google Patents
Water-phase synthesis method for water-soluble CdZnTe ternary quantum dots Download PDFInfo
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- CN101235289A CN101235289A CNA2008100330059A CN200810033005A CN101235289A CN 101235289 A CN101235289 A CN 101235289A CN A2008100330059 A CNA2008100330059 A CN A2008100330059A CN 200810033005 A CN200810033005 A CN 200810033005A CN 101235289 A CN101235289 A CN 101235289A
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Abstract
The invention relates to an aqueous phase synthesis process of water-soluble CdZnTe ternary quantum dots in the nano technology field. The invention chooses oxide of cadmium salt or cadmium as cadmium source, oxide of zinc salt or zinc as zinc source and sodium hydrogen telluride formed by tellurium powder and sodium borohydride, uses sulfhydryl group compound as stabilizer, and prepares the mixing solution of Cd, Zn precursor solution under the protection of nitrogen, and obtains water-soluble CdZnTe ternary quantum dots through reacting after adding sodium hydrogen telluride under the condition of heating reflux. The sulfhydryl peptides substance is used as stabilizer in the invention, thereby obtaining the CdZnTe ternary quantum dots which have excellent stability and high fluorescent property. The invention can obtain water-soluble CdZnTe ternary quantum dots which have excellent dispersibility, uniform grain size and favorable fluorescent property under the mild reaction condition through adopting water solution preparation process and heating with oil bath companying with fully agitation.
Description
Technical field
The present invention relates to a kind of synthetic method of field of nanometer technology, be specifically related to a kind of water phase synthesis method of water-soluble CdZnTe ternary quantum dots.
Background technology
Semiconductor-quantum-point is because its distinctive quantum size effect and surface effects, have many advantages with respect to traditional luminescent dye molecule as marker: spectral width, the emmission spectrum of exciting light are narrow, symmetrical, the fluorescent emission wavelength can be by changing quantum dot size and component and being regulated, therefore the quantum dot of different size can be launched the fluorescence of different colours by the optical excitation of single wavelength, can be used for the multi-color marking of multiple goal molecule.In addition, the luminous intensity height of quantum dot, photochemical stability is good, therefore not only purposes is widely arranged, go out wide application prospect in biomedical fields such as molecular biology, immunobiology, clinical medicine in optoelectronic information fields such as photoelectric device, photodiode, solid luminescence devices.
The semiconductor-quantum-point that is applied to field of biology has excellent luminescent properties (high fluorescence quantum efficiency and narrow fluorescence spectrum halfwidth) except needs, and it is water-soluble also to require it to have.Therefore, the water-soluble semiconductor-quantum-point of preparing excellent in optical properties becomes the research focus of quantum dot preparation in recent years.In recent years, the preparation of water-soluble quantum dot relates to the compound of II-VI and III-V subgroup mostly, is majority with binary quantum dot or binary nuclear shell structure quantum point wherein, and aqueous phase synthesis of ternary quantum dot is then less relatively.
Find through literature search prior art, the people such as Z.Yang of Singapore's biotechnology and nanosecond science and technology association have delivered " Aqueous Synthesis of Glutathione-Capped ZnSe and Zn at " Advanced Materials " (" advanced material ", 2007 19 volume 1475-1479 pages or leaves)
1-xCd
xSe AlloyedQuantum Dots (" ZnSe and the Zn of gsh parcel
1-xCd
xThe water method of Se alloy-type quantum dot is synthetic "), adopted following preparation method in this article: reflux ZnSe precursor solution under 95 ℃ of conditions obtains the ZnSe quantum dot of emission wavelength from 350～370 nanometers by changing the different reaction times; And in resulting ZnSe quantum dot solution, add the Cd precursor solution again, and continue the reflux mixing solutions afterwards, by changing different reaction times and different Cd/Zn ratios, obtain the Zn of emission wavelength from 430～470 nanometers
1-xCd
xThe Se ternary quantum dots.In this system, adopt the part of gsh, and can regulate its emission wavelength, for example the Zn that obtains in the document by changing the Cd/Zn ratio as quantum dot
0.75Cd
0.25Se, Zn
0.62Cd
0.38Se, Zn
0.4Cd
0.6The Se emission wavelength is respectively 428nm, 448nm, and 474nm, its quantum yield is respectively 20%, 31%, and 50%.But the preparation that a remarkable shortcoming of this method is this ternary quantum dots need divide two stages to carry out, promptly need be at the basic enterprising one-step synthesis CdZnSe quantum dot of preparation ZnSe quantum dot, and obtaining the performance of ZnSe quantum dot, will the CdZnSe quantum dot performance of further acquisition be exerted an influence the fs, as fluorescence quantum efficiency, fluorescent emission peak width and its defective that may exist etc. of ZnSe quantum dot.
Summary of the invention
The present invention is directed to the deficiency of the water synthesis technical field of existing ternary quantum dots, a kind of water phase synthesis method of water-soluble CdZnTe ternary quantum dots is provided, make the one step prepare water-soluble CdZnTe ternary quantum dots, simple and the mild condition of reactions steps, the water-soluble CdZnTe ternary quantum dots of acquisition has good dispersiveness, particle size uniformity and high fluorescence quantum efficiency.
The present invention is achieved through the following technical solutions: the oxide compound of selecting cadmium salt or cadmium for use is the cadmium source; the oxide compound of zinc salt or zinc is the zinc source; the sodium hydrogen telluride that tellurium powder and sodium borohydride form is the tellurium source; with the sulfhydryl compound is stablizer; under nitrogen protection, make the mixing solutions of Cd, Zn precursor solution; and under the reflux condition, react after injecting sodium hydrogen telluride therein, obtain water-soluble CdZnTe ternary quantum dots.
The inventive method comprises three steps:
(a) preparation is as the sodium hydrogen telluride NaHTe solution in tellurium source.
With tellurium powder Te and sodium borohydride NaBH
41/2.2 mixes the back and adds 1 ml deionized water in molar ratio, 30 ℃ of standing and reacting 2 hours, makes Te precursor solution NaHTe solution.
(b) preparation Cd
2+, Zn
2+The mixing solutions of precursor solution
With the oxide compound of oxide compound, zinc salt or the zinc of cadmium salt or cadmium and sulfhydryl compound by (Cd
2++ Zn
2+)/sulfydryl mol ratio 1: 2.5, Cd
2+/ Zn
2+Mol ratio 0.4: 1～2.5: 1 mix be dissolved in be mixed with in the deionized water Cd ionic concn 4 mmoles/liter precursor solution, and regulator solution pH value is 9.0.Logical nitrogen is 30 minutes in the mixing solutions of Cd, Zn precursor solution.
(c) preparation CdZnTe ternary quantum dots
Then NaHTe solution is pressed (Cd
2++ Zn
2+)/Te
2-Mol ratio was injected mixing solutions in 3: 1～7: 1, heated in 95 ℃ oil bath 1～6 hour, and accompanied by abundant stirring, obtained water-soluble CdZnTe ternary quantum dots.
The oxide compound of described cadmium salt or cadmium, oxyhydroxide are Cadmium chloride fine powder, Cadmium oxide, cadmium hydroxide, cadmium iodide, Cadmium Sulfide, cadmium nitrate, cadmium perchlorate, cadmium chlorate, Cadmium Sulphate, cadmium acetate or cadmium carbonate.
The oxide compound of described zinc salt or zinc, oxyhydroxide are zinc chloride, zinc oxide, zinc hydroxide, zinc iodide, zinc sulphide, zinc nitrate, zinc perchlorate, zinc chlorate, zinc sulfate, zinc phosphate, zinc oxalate, zinc acetate or zinc carbonate.
Described sulfhydryl compound comprises: a kind of in sulfydryl peptides, mercapto-amine compounds, mercaptan acid compounds or the sulfur alcohol compound.
Described sulfydryl peptides is gsh or thio chitosan; Described mercapto-amine compounds is mercaptoethylamine, sulfydryl propylamine, sulfydryl butylamine, sulfydryl b ammonium salt, sulfydryl third ammonium salt or sulfydryl fourth ammonium salt; Described mercaptan acid compounds is Thiovanic acid or thiohydracrylic acid; Described sulfur alcohol compound is mercaptoethanol or thioglycerol and derivative thereof.
The method reactions steps of the water-soluble CdZnTe ternary quantum dots that the present invention makes is simple, mild condition, easy to operate.Can obtain the CdZnTe quantum dot of different emission by the different reactant ratio of control, reaction times.Resulting CdZnTe quantum dot fluorescence performance is stronger, and the fluorescent emission wavelength region is 487～600 nanometers, and the halfwidth of fluorescence emission peak is 38～60 nanometers, and fluorescence quantum efficiency can reach 70%.
Description of drawings
Fig. 1 is the ultraviolet-visible absorption spectroscopy and the fluorescence emission spectrogram of the water-soluble CdZnTe quantum dot of preparation among the embodiment 1.
Fig. 2 is the ultraviolet-visible absorption spectroscopy and the fluorescence emission spectrogram of the water-soluble CdZnTe quantum dot of preparation among the embodiment 2.
Fig. 3 is the ultraviolet-visible absorption spectroscopy and the fluorescence emission spectrogram of the water-soluble CdZnTe quantum dot of preparation among the embodiment 3.
Fig. 4 is the ultraviolet-visible absorption spectroscopy and the fluorescence emission spectrogram of the water-soluble CdZnTe quantum dot of preparation among the embodiment 4.
Embodiment
The present invention will be further described below in conjunction with example.Present embodiment has provided detailed embodiment and process being to implement under the prerequisite with the technical solution of the present invention, but protection scope of the present invention is not limited to following embodiment.
Embodiment 1
(a) synthetic sodium hydrogen telluride NaHTe solution
With 20 milligrams of Te powder and 13 milligrams of sodium borohydride NaBH
4Powder mixes is put into 5 ml sample bottles and is added 1 ml deionized water, and then reaction flask being placed temperature is reaction 2 hours under 30 ℃ the condition, promptly obtains NaHTe solution.
(b) preparation Cd
2+, Zn
2+Precursor solution
In there-necked flask, add 80 ml deionized water, successively add 73 milligrams of CdCl
22.5H
2O, 109 milligrams of ZnCl
2With 860 milligrams of gsh, obtain (Cd
2++ Zn
2+)/GSH mol ratio is 1: 2.5, Cd
2+/ Zn
2+Mol ratio 2: 5, Cd
2+Concentration 4 mmoles/liter Cd
2+, Zn
2+Precursor solution, and regulator solution pH value is 9.0, feeds nitrogen 30 minutes afterwards in solution.
(c) aqua-solution method prepares the CdZnTe quantum dot
The front is prepared NaHTe inject the Cd for preparing above
2+/ Zn
2+In-GSH the precursor solution, obtain (Cd
2++ Zn
2+)/Te
2-7: 1 CdZnTe precursor solution of mol ratio places solution 95 ℃ of oil baths to heat 4 hours respectively then, and accompanies by abundant stirring, promptly obtains the stable CdZnTe quantum dot of gsh.As shown in Figure 1, preparation-obtained CdZnTe quantum dot fluorescence emission wavelength is 534 nanometers, and the halfwidth of fluorescence emission peak is 54 nanometers, and quantum yield is 28.5%.
Embodiment 2
(a) synthetic sodium hydrogen telluride NaHTe solution
With 20 milligrams of Te powder and 13 milligrams of sodium borohydride NaBH
4Powder mixes is put into 5 ml sample bottles and is added 1 ml deionized water, and then reaction flask being placed temperature is reaction 2 hours under 30 ℃ the condition, promptly obtains NaHTe solution.
(b) preparation Cd
2+, Zn
2+Precursor solution
In there-necked flask, add 57 ml deionized water, successively add 52 milligrams of CdCl
22.5H
2O, 78 milligrams of ZnCl
2With 615 milligrams of gsh, obtain (Cd
2++ Zn
2+)/GSH mol ratio is 1: 2.5, Cd
2+/ Zn
2+Mol ratio 2: 5, Cd
2+Concentration 4 mmoles/liter Cd
2+, Zn
2+Precursor solution, and regulator solution pH value is
9.0, exceedingly high nitrogen 30 minutes in solution afterwards.
(c) aqua-solution method prepares the CdZnTe quantum dot
The front is prepared NaHTe inject the Cd for preparing above
2+/ Zn
2+In-GSH the precursor solution, obtain (Cd
2++ Zn
2+)/Te
2-5: 1 CdZnTe precursor solution of mol ratio places solution 95 ℃ of oil bath heating 4 hours then, and accompanies by abundant stirring, promptly obtains the stable CdZnTe quantum dot of gsh.As shown in Figure 2, preparation-obtained CdZnTe quantum dot fluorescence emission wavelength is 547 nanometers, and the halfwidth of fluorescence emission peak is 59 nanometers, and quantum yield is 37.9%.
Embodiment 3
(a) synthetic sodium hydrogen telluride NaHTe solution
With 20 milligrams of Te powder and 13 milligrams of sodium borohydride NaBH
4Powder mixes is put into 5 ml sample bottles and is added 1 ml deionized water, and then reaction flask being placed temperature is reaction 2 hours under 30 ℃ the condition, promptly obtains NaHTe solution.
(b) preparation Cd
2+, Zn
2+Precursor solution
In there-necked flask, add 115 ml deionized water, successively add 104 milligrams of CdCl
22.5H
2O, 46 milligrams of ZnCl
2With 615 milligrams of gsh, obtain (Cd
2++ Zn
2+)/GSH mol ratio is 1: 2.5, Cd
2+/ Zn
2+Mol ratio 4: 3, Cd
2+Concentration 4 mmoles/liter Cd
2+, Zn
2+Precursor solution, and regulator solution pH value is 9.0, feeds nitrogen 30 minutes afterwards in solution.
(c) aqua-solution method prepares the CdZnTe quantum dot
The front is prepared NaHTe inject the Cd for preparing above
2+/ Zn
2+In-GSH the precursor solution, obtain (Cd
2++ Zn
2+)/Te
2-5: 1 CdZnTe precursor solution of mol ratio places solution 95 ℃ of oil bath heating 1 hour then, and accompanies by abundant stirring, promptly obtains the stable CdZnTe quantum dot of gsh.As shown in Figure 3, preparation-obtained CdZnTe quantum dot fluorescence emission wavelength is 487 nanometers, and the halfwidth of fluorescence emission peak is 45 nanometers, and quantum yield is 11%.
Embodiment 4
(a) synthetic sodium hydrogen telluride NaHTe solution
With 20 milligrams of Te powder and 13 milligrams of sodium borohydride NaBH
4Powder mixes is put into 5 ml sample bottles and is added 1 ml deionized water, and then reaction flask being placed temperature is reaction 2 hours under 30 ℃ the condition, promptly obtains NaHTe solution.
(b) preparation Cd
2+, Zn
2+Precursor solution
In there-necked flask, add 86 ml deionized water, successively add 78 milligrams of CdCl
22.5H
2O, 19 milligrams of ZnCl
2With 369 milligrams of gsh, obtain (Cd
2++ Zn
2+)/GSH mol ratio is 1: 2.5, Cd
2+/ Zn
2+5: 2 Cd of mol ratio
2+, Zn
2+Precursor solution, and regulator solution pH value is 9.0, feeds nitrogen 30 minutes afterwards in solution.
(c) aqua-solution method prepares the CdZnTe quantum dot
The front is prepared NaHTe inject the Cd for preparing above
2+/ Zn
2+In-GSH the precursor solution, obtain (Cd
2++ Zn
2+)/Te
2-3: 1 CdZnTe precursor solution of mol ratio places solution 95 ℃ of oil bath heating 6 hours then, and accompanies by abundant stirring, promptly obtains the stable CdZnTe quantum dot of gsh.As shown in Figure 4, preparation-obtained CdZnTe quantum dot fluorescence emission wavelength is 539 nanometers, and the halfwidth of fluorescence emission peak is 46 nanometers, and quantum yield is 64.5%.
Claims (10)
1, a kind of water solution preparation method of water-soluble CdZnTe ternary quantum dots; it is characterized in that: the oxide compound of selecting cadmium salt or cadmium for use is the cadmium source; the oxide compound of zinc salt or zinc is the zinc source; the sodium hydrogen telluride that tellurium powder and sodium borohydride form is the tellurium source; with the sulfhydryl compound is stablizer; under nitrogen protection, make the mixing solutions of Cd, Zn precursor solution, and under the reflux condition, react after injecting sodium hydrogen telluride therein, obtain water-soluble CdZnTe ternary quantum dots.
2, the water solution preparation method of water-soluble CdZnTe ternary quantum dots as claimed in claim 1 is characterized in that, may further comprise the steps:
(a) preparation is as the sodium hydrogen telluride NaHTe solution in tellurium source
With tellurium powder Te and sodium borohydride NaBH
41/2.2 mixes back adding deionized water in molar ratio, and standing and reacting makes Te precursor solution NaHTe solution;
(b) preparation Cd
2+, Zn
2+The mixing solutions of precursor solution
With the oxide compound of oxide compound, zinc salt or the zinc of cadmium salt or cadmium and sulfhydryl compound by (Cd
2+, Zn
2+)/sulfydryl mol ratio 1: 2.5, the mixing in 0.4: 1～2.5: 1 of Cd/Zn mol ratio are dissolved in and are mixed with precursor solution in the deionized water, regulator solution pH value, logical nitrogen in the mixing solutions of Cd, Zn precursor solution afterwards;
(c) preparation CdZnTe ternary quantum dots
NaHTe solution is pressed the Zn/Te mol ratio injected mixing solutions in 2: 1～5: 1, heat in the oil bath, and accompany by abundant stirring, obtain water-soluble CdZnTe ternary quantum dots.
3, the water solution preparation method of water-soluble CdZnTe ternary quantum dots as claimed in claim 2 is characterized in that, in the step (a): NaHTe solution is by Te powder and NaBH
4After mixing in 1: 2.2 in molar ratio, add 1 ml deionized water, made in 2 hours 30 ℃ of reactions.
4, the water solution preparation method of water-soluble CdZnTe ternary quantum dots as claimed in claim 2 is characterized in that, in the step (b): precursor solution pH value is 9.0, logical nitrogen 30 minutes.
5, as the water solution preparation method of claim 2 or 4 described water-soluble CdZnTe ternary quantum dots, it is characterized in that, in the step (b): in the mixing solutions of Cd, Zn precursor solution the Cd ionic concn be 4 mmoles/liter.
6, the water solution preparation method of water-soluble CdZnTe ternary quantum dots as claimed in claim 2 is characterized in that, in the step (c): heated in 95 ℃ oil bath 1～6 hour.
7, the water solution preparation method of water-soluble CdZnTe ternary quantum dots as claimed in claim 1 or 2, it is characterized in that the oxide compound of described cadmium salt or cadmium, oxyhydroxide are Cadmium chloride fine powder, Cadmium oxide, cadmium hydroxide, cadmium iodide, Cadmium Sulfide, cadmium nitrate, cadmium perchlorate, cadmium chlorate, Cadmium Sulphate, cadmium acetate or cadmium carbonate.
8, the water solution preparation method of water-soluble CdZnTe ternary quantum dots as claimed in claim 1 or 2, it is characterized in that the oxide compound of described zinc salt or zinc, oxyhydroxide are zinc chloride, zinc oxide, zinc hydroxide, zinc iodide, zinc sulphide, zinc nitrate, zinc perchlorate, zinc chlorate, zinc sulfate, zinc phosphate, zinc oxalate, zinc acetate or zinc carbonate.
9, the water solution preparation method of CdZnTe ternary quantum dots as claimed in claim 1 or 2 is characterized in that, described sulfhydryl compound comprises: a kind of in sulfydryl peptides, mercapto-amine compounds, mercaptan acid compounds or the sulfur alcohol compound.
10, the water solution preparation method of water-soluble CdZnTe ternary quantum dots as claimed in claim 9 is characterized in that, described sulfydryl peptides is gsh or thio chitosan; Described mercapto-amine compounds is mercaptoethylamine, sulfydryl propylamine, sulfydryl butylamine, sulfydryl b ammonium salt, sulfydryl third ammonium salt or sulfydryl fourth ammonium salt; Described mercaptan acid compounds is Thiovanic acid or thiohydracrylic acid; Described sulfur alcohol compound is mercaptoethanol or thioglycerol and derivative thereof.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103204634A (en) * | 2013-03-15 | 2013-07-17 | 北京科技大学 | Method for manufacturing semiconductor sulfide biopolymer nano-composite film |
| CN106053823A (en) * | 2016-04-15 | 2016-10-26 | 山东大学 | Spectral electrochemiluminescent immunodetection method based on CdZnSe three-component quantum dots |
-
2008
- 2008-01-24 CN CNA2008100330059A patent/CN101235289A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103204634A (en) * | 2013-03-15 | 2013-07-17 | 北京科技大学 | Method for manufacturing semiconductor sulfide biopolymer nano-composite film |
| CN103204634B (en) * | 2013-03-15 | 2014-12-17 | 北京科技大学 | Method for manufacturing semiconductor sulfide biopolymer nano-composite film |
| CN106053823A (en) * | 2016-04-15 | 2016-10-26 | 山东大学 | Spectral electrochemiluminescent immunodetection method based on CdZnSe three-component quantum dots |
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